Determination of Organic Emission of Non-metallic materials from vehicles Interior VDA 277
Contents
1. General
2. Test preparations
3. Testing sets and conditions
4. Attempt realization
5. Calibration
6. Evaluation
1. General
1.1 Purposes
According to this test method, the organic emission from non-metallic materials is determined with direct or indirect influence for the passenger's cell of automobiles stand. It measure the emission potential of a material, the sum of all release values of the emitted substances with gaschromatograph and detection with a Flame ionization detector. The test operated by means of steam space analysis (Head Space technology) at temperature of 120ºC.
1.2 Requirements
The accompanying sample, the respective requirements as well as special method is of the suitable specification to take drawing or the like.
If materials are composed of different components, a separate check is required for every single material.
2. Test preparations
Transport and storage of the tests has to occur in an aluminum coated Polyethylenbeutel. The sampling has immediately after incoming goods or in a condition, which corresponds to this, to take place. The times of the incoming goods and the sampling are to be labelled. There is no conditioning of the test as a rule. Except of it are physical materials (cotton, wood, leather, wool). These materials are dried before the weighted sample in the chopped up state for 24 hours with calcium chloride (CaCl2).
The test is to be inferred at the agreed place about the whole test cross section from the component. The samples are chopped up in pieces with a weight more than 10 mg and less than 25 mg, without the test warms itself up. If necessary, another test preparations can be also undertaken and such deviation from standard should be mentioned in the final result.
The test amount to be rocked to sleep is directed after the size of the Head Space of little glass whose least contents 5 ml must amount. Per 10 ml little glass volumes are to be rocked to sleep 1.000 g +0.001 g (i.e. maximum content error 0.1%) test material. Metal are to be removed before weighting. When metal parts are liable to organic substances, for example, varnish, pastes, should be separated mechanically at first and then to rock to sleep.
The weighted test particles become in a Head Space little glasses (least 3 little glasses per test), then air-tighted with the use of a septums with the Teflon coating which points to the interior of the little glass.
3. Testing sets and conditions
3.1 testing sets
Gaschromatograph for capillary column with Head Space Tester, flame ionization detector (FID) and calculator/ Integrator.
WCOT-capillary dividing column with a separating phase from 100% Polyethylene glycol (so-called Wax type, e.g., DBWax, Carbowax...)
0.25 mm I.D., 0.25 µm film thickness, 30-m length
Analytic balance, in the order of 0.1 mg
Microliter syringe, 5 µl, sample in vitreous body
3.2 measuring conditions
Stove temperature program GC: 3 minutes isotherm at 50ºC
Heating at 200ºC with a rate of 12 K / min
4 minutes isotherm at 200ºC
Injector temperature: 200ºC
Detector temperature: 250ºC
Split ratio: approx. 1: 20
Carrier gas: helium
Middle carrier gas speed: approx. 22-27 cm /s.
Remark: the substance 2,6-Di-tert-butyl-4-methylphenol (BHT) must show a retention time smaller than 16 minutes.
4. Attempt realization
The little glasses are tempered to the enrichment of the substances in the air standing about the test directly before the measurement 5 hours + 5 minutes with 120 + 1 ºC in the Head Space Tester and are analyzed directly afterwards. At least 3 tests are to be analyzed in each case.
The control value is determined by average signal value of at least 3 measurements with empty test little glasses.
The dosage must run off in all analyses of the tests, the control value and the calibration solution identically and reproduceable.
The separating column must be brought to the bake once per week for 15 minutes at maximum temperature.
5. Calibration
For the quantitative determination of the total carbon emission as well as the amount of special single substances, calibration curve are compared with the method of the external standard.
For the total carbon emission, acetone serves as a calibration substance, for the single substances and the respective materials.
After installation of a new column and after changes in the device a basic calibration with 7 calibration concentration is to be carried out. In addition, a control calibration with at least 3 concentrations has to be carried out at least every 4 weeks.
